Specac Quest User manual

The Quest
Single Reflection ATR Accessory
User Manual
2I-10800-8

The Quest
Single Reflection ATR Accessory
User Manual
2I-10800-8

User Manual
2
The Quest Single Reflection ATR Accessory
P/N GS10800
CONTENTS
1. INTRODUCTION ................................................................................. 3
2. SAFETY CONSIDERATIONS ................................................................. 5
3. CHECKLIST OF CONTENTS .................................................................. 6
4. INSTALLATION USING BENCHMARK ™ BASE LATE ................................ 7
5. ALIGNMENT ROCEDURE FOR QUEST ATR ACCESSORY ........................ 8
FITTING OF QUEST ATR CRYSTAL UCK TO THE O TICAL UNIT ............... 8
FINE ALIGNMENT ............................................................................. 12
SYNO TI - FOCAL MIRROR SYSTEM ..................................................... 13
ALIGNMENT ROCEDURE ................................................................. 14
6. URGING THE QUEST ATR O TICAL UNIT ........................................... 19
FITTING THE URGE BELLOWS ( / N GS10707) ................................. 21
7. QUEST ATR ANVILS AND CLAM ANVIL ARM ASSEMBLY ....................... 22
CHOICE OF ANVILS AND THEIR USES ................................................. 22
CLAM ANVIL ARM ASSEMBLY ........................................................... 23
TORQUE LIMITER SCREW KNOB ASSEMBLY ........................................ 25
8. SAM LING USING THE QUEST ATR ACCESSORY .................................. 26
COLLECTING ATR S ECTRA OF OWDER SAM LES ............................. 27
COLLECTING ATR S ECTRA OF FLAT SOLID SAM LES ......................... 29
COLLECTING ATR S ECTRA OF ELLET / BEAD SAM LES ...................... 30
COLLECTING ATR S ECTRA OF FIBER SAM LES ................................. 31
COLLECTING ATR S ECTRA OF LIQUID AND ASTE SAM LES ............... 33
THE VOLATILES COVER ( / N GS10825) ............................................ 34
THE S ECULAR REFLECTANCE UCK ( / N GS10816) ........................ 36
NOTES ON CLEANING ....................................................................... 38
9. QUEST ATR ACCESSORY ART IDENTIFICATION LIST ........................... 44
10. QUEST ATR ACCESSORY S ARE ARTS ........................................... 45
11. QUEST ATR TECHNICAL S ECIFICATIONS ......................................... 46
12. QUEST ATR SERIAL NUMBERS ......................................................... 47
© February 2018 Specac Ltd. All rights reserved.
Benchmark and Brilliant Spectroscopy are trademarks of Specac Ltd.
Other product names mentioned herein may be trademarks
of their respective owners.

Quest Single Reflection ATR Accessory
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1. ntroduction
Thank you for buying a Specac product. We trust it will provide you
with invaluable and excellent service in use.
The Quest Single Reflection ATR Accessory is designed for the
quantitative and qualitative analysis of solids, powders, liquids, pastes
and gum-like samples using Mid IR spectroscopy at ambient
temperature and pressure conditions. rincipally, ATR spectral
measurements at a nominal 45° incident angle are made, but specular
reflectance measurements at the same nominal incident angle can be
made using an optional specular reflectance puck assembly. Sufficient
sample is required to cover an ATR crystal surface offered from a
single crystal diamond, zinc selenide (ZnSe), germanium (Ge) and
silicon (Si) flat crystal top plate assembly (puck) options.
The Quest ATR Accessory is based upon Synopti-Focal technology –
an innovative synoptic focusing array of highly reflective gold coated
mirror only optics – in an optical unit that supports the interchangeable
ATR crystal puck assemblies. An IR light beam that is projected
towards the ATR crystal is presented at a nominal 45° angle of
incidence to the sample surface. As the optical unit of the Quest ATR
Accessory consists of mirrors as reflective components only, it allows
for as wide a range as possible of the spectral frequency throughput
for the specific ATR crystal puck assembly being used. For mid IR
spectral data the typical spectral range that can be collected for the
different ATR crystal puck types are as follows:
Diamond puck – 7,800cm-1 to 400cm-1 (AR coated crystal).
Diamond puck – 10,000cm-1 to 40cm-1 (Extended Range – non-AR
coated crystal).
ZnSe puck – 7,800cm-1 to 500cm-1. (AR coated crystal).
Germanium puck – 5,500cm-1 to 480cm-1. (AR coated crystal).
Silicon puck – 8,333 to 100cm-1. (Non-AR coated crystal).
As mentioned, there is also an option in use of the Quest ATR
Accessory for the spectral measurement of solid sample types such as
flat surface films by the specular reflectance technique. The ATR

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crystal puck assembly is replaced with a puck assembly that has no
ATR crystal fitted to allow for the nominal 45° incident angle of light to
be projected directly to the solid sample surface.
An adjustable clamp arm assembly with a set load torque limiter screw
knob is permanently affixed to the optical unit. There is a choice of self-
levelling flat or concave pellet compression head anvils to use with the
clamp arm assembly depending upon the sample type to be studied
using an ATR crystal puck assembly. (No anvil is used for specular
reflectance measurements of solid sample types.) The torque limiter
screw knob provides for a consistent and reproducible load to either
one of the flat or pellet anvils to enable excellent close contact of a
solid sample with the ATR crystal. In operation, the entire torque screw
knob is rotated until a sufficient load and hence pressure has been
applied to the sample. The torque screw knob will continue to rotate
when the set load is reached, but the drive connection slips and no
more force will be applied. A “clicking” sound with continual rotation of
the knob acts as the indicator when the set applied load has been
reached. When using the clamp arm assembly with a compression
head anvil for pressure application to solid sample types, the anvil
does not rotate against the sample. This ensures that heat is not
generated by friction which may cause changes to the sample, and the
sample is not displaced from the correct sampling position.
The optical unit of the Quest ATR Accessory can be supplied in a
variety of different top surface colours on a light grey optical unit. The
standard colour is black (B), but there are options of red (R), yellow
(Y), orange (O), green (G), aqua (A) and purple ( ).
Quest ATR Accessory

Quest Single Reflection ATR Accessory
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2. Safety Considerations
With use of any spectroscopic accessory that involves the study of a
wide range of chemical samples, the associated risk in handling may
mostly be attributed to the specific sample type to be handled itself. As
far as it is possible you should follow a procedure for safe handling and
containment of the type of sample to be used.
With respect to safety of use specifically to the Quest ATR Accessory,
this uses different crystal materials for the ATR crystal puck
assemblies where a sample is bought into contact for analytical
spectroscopic study. As standard, Diamond (type IIIA), Germanium
(Ge), Zinc Selenide (ZnSe) and Silicon (Si) are the four crystal
materials of choice that can be used.
Caution: Out of these four different crystal types, ZnSe is
the most potentially hazardous material with respect to
toxicity risk in use and handling.
Diamond, Ge and Si crystal materials can be considered relatively safe
to use, although Ge and Si may be harmful to the body if ingested in
significant quantity. The general rule when working with any crystal
material (and sample) is to always wear gloves and safety gear (e.g.
safety spectacles) when handling to obviate the risk of contact with the
skin.
rovided with each crystal version of puck assembly is a window
material safety data sheet for the crystal material itself that can be
consulted for safe handling. A copy of each of these datasheets can
also be found in this Quest instruction manual in the Notes On
Cleaning Section found on pages, 40, 41, 42 and 43.

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3. Checklist of Contents
The Quest ATR Accessory is provided in its own specific packaging.
Depending on which Quest ATR system (the colour of the optical unit
and a specific crystal puck assembly), has been ordered will determine
the items to check on delivery.
lease check for the following.
1 Quest ATR Accessory including optical unit (with top surface colour
of choice) and clamp arm and anvil assembly.
1 Stainless steel flat anvil /N GS10820.
1 Stainless steel pellet anvil /N GS10821.
1 air of purge bellows /N GS10707.
1 Volatiles cover /N GS10825.
1 ATR crystal puck assembly (choice of Diamond, ZnSe, Ge or Si
crystal puck assembly).
Any additional Quest ATR crystal pucks or specular reflectance puck
ordered with the accessory.
1 Ball driver 3.0mm (for optical unit cover plate removal).
1 Ball driver 2.5mm (for mirror adjustment in optical unit).
1 Benchmark™ baseplate for your FTIR spectrometer.
1 Instruction manual for Benchmark™ baseplate installation.
1 Instruction manual for Quest ATR Accessory.
1 Quickstart guide for Quest ATR Accessory.
Carefully remove your Quest ATR Accessory and ATR crystal puck
assembly(s) from the packaging in readiness for use.

Quest Single Reflection ATR Accessory
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4. nstallation Using Benchmark™ Baseplate
Fig . Quest ATR Accessory – Optical Unit with Clamp Arm/Anvil
Assembly and ATR Crystal Puck Assembly
The Quest ATR Accessory is supported on a Benchmark™ baseplate
when installed into a spectrometer. The Benchmark™ baseplate
typically has three support pillars (one flat support pillar towards the
rear and two at the front with location pins) and a fourth front central
pillar into which the fixing thumb screw ( ) of the Quest ATR optical
unit is tightened.
Note: It is normally best to install the Benchmark baseplate in
the spectrometer first before locating the Quest ATR
Accessory.
Fixing holes and studs in the Benchmark™ baseplate will vary
dependent upon the make and model of the spectrometer into which
the Quest ATR Accessory is to be installed. For details on how to
install your accessory in the spectrometer, refer to the Benchmark™
baseplate Installation Guide/User Manual supplied.

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5. Alignment Procedure for Quest ATR
When you have installed the Quest ATR Accessory into your
spectrometer on its appropriate Benchmark™ baseplate, you should
check for alignment of the accessory. An overall spectral throughput of
light energy between 10% and 35%, dependent upon the ATR crystal
puck assemblies and spectrometer used should be achievable. The
Quest ATR Accessory with your choice of crystal puck will be supplied
having a preliminary factory alignment. On installation, some
transmitted energy should be recorded on the spectrometers
energy/light detector monitoring system, but it will be necessary to
maximize the optical throughput for any specific spectrometer by
adjusting the mirrors in the optical unit of the Quest ATR Accessory. To
carry out any alignment procedure one of the Quest ATR flat crystal
puck assemblies must be fitted to the optical unit.
Fitting of the Quest ATR Crystal Puck to the Optical Unit
Seven different versions of Quest ATR crystal puck assemblies can be
fitted to the optical unit. They are:
Quest ATR Diamond crystal puck, /N GS10810.
Quest ATR Diamond extended range crystal puck, /N GS10811.
Quest ATR ZnSe crystal puck, /N GS10812.
Quest ATR Ge crystal puck, /N GS10813.
Quest ATR Si crystal puck, /N GS10819.
Quest ATR Diamond crystal puck with diamond like carbon (DLC)
coating, /N GS10826.
Quest ATR Diamond extended range crystal puck with diamond like
coating (DLC), /N GS10827.
The ATR crystals of these puck assemblies have an antireflection (AR)
coating on their underside surfaces for improved light throughput
characteristics, except the extended range diamond crystal pucks
/N’s GS10811 and GS10827, and the silicon puck /N GS10819.
Serial number and puck crystal identification labels are affixed to the
underside surface of the puck assembly. (A note of the serial number
of your crystal puck assembly can be made on page 47 of this user
instruction manual for your reference records.)

Quest Single Reflection ATR Accessory
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Diamond Like Carbon (DLC) Coating on Puck Assemblies
The two diamond AR coated and extended range crystal puck
assembly options as /N’s GS10826 and GS10827 are provided with a
protective DLC coating over the surrounding stainless steel circular
puck top surface to the ATR crystal.
Note: The diamond ATR crystals of these Quest ATR crystal puck
assemblies do not have a DLC coating applied to the surface.
The DLC coating is a durable, chemically resistant layer of 7 microns
thickness covering the stainless steel puck surface. The diamond ATR
crystal itself used in the puck assembly for any spectral analysis from
actual sample contact is a highly chemically inert substance,
impervious to attack from a very wide range of chemical types that can
be studied. Applying an additional DLC coating protective layer to the
surrounding and supporting stainless steel puck of the diamond ATR
crystal extends the chemical resistance properties of the puck
assembly overall. Typically, 1 mol/L concentration hydrochloric acid
solution (HCL – pH0) and 1 mol/L concentration sodium hydroxide
solution (NaOH – pH14) have little or no effect when contacting the
DLC coated stainles steel puck assembly surface continuously for an
hour at ambient conditions.
Quest ATR Crystal Puck Assemblies Identification
Top and underside views of the Quest ATR crystal puck assemblies
using the diamond crystal puck /N GS10810 as an example are
shown as Figs 2 and 3. (ZnSe, Ge and Si top plates are similar.)
The top surface area of the Quest ATR optical unit for positioning of
the ATR crystal pucks, is shown as Fig 4.

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Fig 2. Top view of Quest ATR Diamond Crystal
Puck Assembly
Fig 3. Underside view of Quest ATR Diamond Crystal
Puck Assembly
Note: The fixing nuts for the underside support bracket of the puck
assembly will be covered with tamperproof red marking strips
and these fixing nuts should never be touched. Any attempt to
adjust these nut fixings will be identifiable and will invalidate any
warranty for the puck assembly.
ATR Crystal
2
ATR
Crystal
Serial Number Label
Crystal Puck
Identification Label

Quest Single Reflection ATR Accessory
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Fig 4. Top view of Quest ATR Optical Unit showing location area
for the Crystal Puck Assemblies
The ATR crystal puck assemblies will fit onto the top surface area of
the Quest ATR Accessory in one orientation only. Align the location
slot (notch) (2) on the underside of the crystal puck (see Fig 3.) with
the location pin (3). The location slot (2) of the ATR crystal puck must
be facing towards the front of the Quest ATR Accessory where the
thumbscrew fixing ( ) is located. (See Fig .) Allow the three magnetic
circular spot catches (4) to engage to the underside circumference
surface of the ATR crystal puck to hold it securely in position. To
remove and swap over with any other ATR crystal puck assembly, just
grip the sides of the ATR crystal puck and pull it up to release the hold
of the magnetic catches.
3
4

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Fine Alignment
With a Quest ATR crystal puck assembly in position on the optical unit
and when this completed assembly is installed in the spectrometer on
an appropriate Benchmark™ baseplate, the Quest ATR Accessory can
be finely aligned. The optical unit front cover plate (5) is removed by
undoing the two captive cover plate screws (6) (see Fig 5.) using the
3mm ball driver supplied. The front cover plate (5) is pulled up and
forward over the fixing thumb screw ( ) for its removal to gain access
to the internal mirrors for adjustment.
Fig 5. Quest ATR - Front Cover Plate Removal
5
6

Quest Single Reflection ATR Accessory
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Synopti-Focal Mirror System
The Quest ATR Accessory is based upon Synopti-Focal technology
which uses an innovative synoptic focusing array of highly reflective
gold coated mirrors for the optical pathway when a different ATR
crystal puck assembly is positioned for use on the optical unit. The
mirror arrangement for an IR beam passage through the Quest ATR
Accessory can be seen from the cutaway front view in Fig 6.
Fig 6. Cutaway front view of Quest ATR Accessory showing the
Synopti-Focal arrangement of mirror components
M5 M4
M6 M3 M M2
ATR Crystal Puck Assembly on Top Plate
S D

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The Quest ATR Accessory can be used in any standard spectrometer
system irrespective of the beam direction of light through the sample
compartment from source to detector. However, for explanation of the
internal IR beam passage through the Quest ATR Accessory the
sequential labeling of mirror components has been assigned for a
spectrometer that has an IR beam running through the sample
compartment from a source (S) on the right-hand side towards a
detector (D) on the left-hand side. For this right to left beam passage
configuration the IR beam sequence is as follows:
S, M , M2, M3, M4 – ATR Crystal – M5, M6, D.
The mirrors M , M2, M3 and M6 are flat, gold coated mirrors. (M6 is a
slightly larger sized mirror, wider and longer than the M , M2 and M3
mirrors, to eliminate any potential stray light throughput.) Mirrors M4
and M5 are aspheric, focusing gold coated mirrors. The angle of
incidence for the IR light beam when it interacts at the crystal/sample
interface surface is nominally set at 45° for the ATR effect.
Alignment Procedure
When the front cover plate (5) has been removed (see Fig 5.) to gain
access to the internal M , M2, M3 and M6 flat mirrors frame assembly,
the mirrors M , M3 and M6 only in the optical unit can be adjusted for
rotation and tilt for alignment, to optimise the light throughput of the
Quest ATR Accessory for your spectrometer system.
Note: The flat mirror M2 and the hemispherical mirrors M4 and M5 do
not require adjustment for the alignment procedure. A cover has
been placed over the rotation adjustment screw for mirror M2
(see Fig 6.) to prevent access for accidental movement.
A 2.5mm ball driver tool has been supplied for adjustment of the
rotation and tilt screws for the mirrors M , M3 and M6. lease refer to
Fig 7. which identifies the rotation and tilt screws that need to be
adjusted for the mirrors M , M3 and M6.

Quest Single Reflection ATR Accessory
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Fig 7. Access to Mirrors M , M3 and M6 - Cover Plate Removed
The grub screw (7) allows for rotation of the M6 mirror and the cap
head screw (8) allows for tilt of the M6 mirror, as fitted to the main
mirror frame assembly.
The grub screw (9) allows for rotation of the M3 mirror and the cap
head screw ( 0) allows for tilt of the M3 mirror, as fitted to the main
mirror frame assembly.
The grub screw ( ) allows for rotation of the M mirror and the cap
head screw ( 2) allows for tilt of the M mirror, as fitted to the main
mirror frame assembly.
M6 M
7 8 2
9 0 M3

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To begin any alignment, first establish that there is a throughput of IR
light radiation passing through the system from (S)ource to (D)etector
with the Quest ATR Accessory installed correctly on it baseplate in the
spectrometer sample compartment and with an ATR crystal puck
assembly in position on the optical unit.
1. Using the 2.5mm ball driver tool (supplied), the alignment
procedure initially involves rotational movement of the mirrors M6,
M3 and M in this sequential order. The grub screws, (7), (9) and
() are turned to make the rotational adjustment for each mirror.
One at a time, very gently rotate each screw, (7), then (9) and
finally ( ), clockwise or anticlockwise to achieve a maximum
energy signal reading. If you travel through a maximum energy
position by, say, continued clockwise rotation, then turn the screw
anticlockwise to bring back to the maximum point again. (And vice
versa).
2. Having achieved a maximum throughput reading from rotation of
the M6, M3 and M mirrors from step 1, now use the 2.5mm ball
driver tool in the cap head screws (8), ( 0) and ( 2) in turn for
these three mirrors (in the same sequence) for their tilt adjustment
position by turning the screws similarly clockwise or anticlockwise
to maximise the energy.
Having optimised all three mirrors M6, M3 and M for both their
rotation and tilt settings for optical alignment, there is likely to be an
overall improvement in the light throughput energy value for the Quest
ATR accessory. Specac would recommend though that a second
“iteration” or sequence of rotation and tilt adjustments for these three
mirrors is carried out to optimize the energy throughput further for the
Quest ATR Accessory. Therefore, repeat the mirror adjustment steps 1
and 2 again.
When satisfied after one (or two) adjustment sequences have been
carried out that an acceptable throughput energy has been
established, the alignment procedure has been completed and the
front cover plate (5) can be repositioned onto the optical unit.

Quest Single Reflection ATR Accessory
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For some spectrometer configurations, if the Benchmark™ baseplate
is mounted on a rail or is movable in the spectrometer, then an overall
energy throughput may be improved by moving the Quest ATR
Accessory on the Benchmark™ baseplate to find the best position
where the transmission energy throughput is at a maximum. Firmly
secure the Benchmark™ baseplate with the Quest Accessory into this
new position if an improvement has been gained.
Note: In some spectrometers it may be necessary to remove the
Quest ATR optical unit before securing the baseplate. Where
this is the case, ensure that the Benchmark baseplate does
not move when removing the Quest ATR optical unit.
Procedure to Follow from Any Accidental Mis-Alignment
During an alignment, if a mistake is made and no signal response from
the detector of the spectrometer can be obtained, then it may be
possible to recover the situation for a partial, visual rough re-alignment
of the mirror optics M , M3 and M6. This will re-establish a small
energy level through the system to reach the detector and allow for the
correct alignment procedure to be followed again to optimise the light
throughput.
Note: The following procedure can also be adopted if any Quest ATR
Accessory to be used is ever found to be out of alignment when
installed into a spectrometer system and there is no register of
an energy throughput to the detector. Mirror M2 should never
need to be adjusted in any alignment procedure.
1) With the front cover plate (5) removed from the optical unit to gain
access to the mirror frame assembly, also remove any crystal puck
assembly from the top of the optical unit and remove the Quest
optical unit from the Benchmark™ baseplate.
2) Using the 2.5mm ball driver tool in the screws (8), ( 0) and ( 2),
adjust all three mirrors M , M3 and M6 ONLY for their angle of tilt
such that these mirror surfaces are normal (i.e. at a 90° right angle)
with relation to the back plane of the main mirror mount frame
assembly affixed to the rear of the optical unit.

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3) Using the 2.5mm ball driver tool in the grub screw (9) to rotate mirror
M3 and in the grub screw ( ) to rotate the mirror M , adjust both
mirrors to form a straight line for both of their mirror surfaces. Refer
to Fig 6 to indicate how they need to be roughly aligned to form a
straight line orientation.
4) Mirror M6 now needs to be adjusted for its rotation using the 2.5mm
ball driver in the grub screw (7) such that its surface is similar in
angular relation to the straight line formed by the two mirrors M3 and
M as seen at Fig 6. An indication that a correct rotational angle for
mirror M6 has been achieved is when the grub screw (7) is proud of
its mirror carriage frame assembly housing by circa 2mm. This depth
indication for the grub screw (7) position can be observed looking
through the aperture port ( 6) on the left-hand side of the optical
unit.
5) With the three mirrors M , M3 and M6 now roughly positioned for
their tilt and rotation angles, the optical unit can be placed back onto
the Benchmark™ baseplate and the crystal puck assembly is
repositioned on top of the optical unit to complete a beam path for
light to travel through the Quest ATR accessory.
6) Set up the IR spectrometer to record an energy throughput level at
the detector. Having followed steps 2) to 5) from the procedure
above, there should now be some energy level indication (however
small), at the detector after passage of light through the Quest ATR
Accessory and so the correct fine alignment procedure can now be
followed starting with further rotation of mirror M6 as described from
step 1) on page 16 of this instruction manual. However, even if there
is still no signal after the procedural steps 2) to 5) have been
completed (pages 17 and 18), then turning the grub screw (7) for
rotation of the mirror M6 (first one way and then the other), at this
stage now should lead to the energy level signal returning and for
progression to an optimum alignment.